CN117996011A - Negative electrode active material, negative electrode, and rechargeable lithium battery - Google Patents
Negative electrode active material, negative electrode, and rechargeable lithium battery Download PDFInfo
- Publication number
- CN117996011A CN117996011A CN202311347951.1A CN202311347951A CN117996011A CN 117996011 A CN117996011 A CN 117996011A CN 202311347951 A CN202311347951 A CN 202311347951A CN 117996011 A CN117996011 A CN 117996011A
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- China
- Prior art keywords
- active material
- negative electrode
- silicon
- lithium battery
- carbon
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 51
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- 229910052799 carbon Inorganic materials 0.000 claims abstract description 20
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- 239000011230 binding agent Substances 0.000 claims description 21
- 239000003792 electrolyte Substances 0.000 claims description 15
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical class [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 abstract description 4
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Classifications
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
Disclosed are a negative electrode active material for a rechargeable lithium battery, a negative electrode including the negative electrode active material, and a rechargeable lithium battery including the negative electrode active material. The negative electrode active material includes: silicon-carbon composites in which crystalline carbon, silicon particles, and amorphous carbon are agglomerated; and single-walled carbon nanotubes coated on the silicon-carbon composite.
Description
Technical Field
Embodiments of the present disclosure relate to a negative electrode active material for a rechargeable lithium battery, and a negative electrode and a rechargeable lithium battery including the same.
Background
Recently, rapid popularization of electronic devices using batteries, such as mobile phones, laptop computers, and electric vehicles, requires a dramatic increase in demand for rechargeable batteries having relatively high capacity and lighter weight. In particular, since the rechargeable lithium battery has a light weight and a high energy density, the rechargeable lithium battery has recently attracted attention as a driving power source for portable devices. Accordingly, research and development to improve the performance of rechargeable lithium batteries are actively being conducted.
The rechargeable lithium battery includes positive and negative electrodes, which may include active materials capable of intercalating and deintercalating lithium ions, and an electrolyte, and generates electric energy due to oxidation and reduction reactions when lithium ions are intercalated and deintercalated into the positive and negative electrodes.
As the positive electrode active material of the rechargeable lithium battery, transition metal compounds such as lithium cobalt oxide, lithium nickel oxide, and lithium manganese oxide are mainly used. As the anode active material, a carbonaceous material such as a crystalline carbon-based material (such as natural graphite or artificial graphite) or an amorphous carbon-based material may be mainly used, but the carbonaceous material has a low capacity of 360mAh/g, and thus, research on a silicon-based active material (such as Si) having a capacity of four times or more has been actively conducted.
However, during charge and discharge, the silicon-based active material has a higher volume expansion (about 300%) than that of a carbon-based material such as graphite, which results in deterioration due to consumption of electrolyte, and thus, it is limited to practical use. Repeated volume expansion and contraction of the silicon-based active material breaks the conductive network, resulting in deterioration of cycle life characteristics.
In order to solve such problems, studies on nano-sizing of silicon-based active materials or recombination into secondary particles by agglomerating silicon and carbon have been conducted, but it is difficult to completely solve the problems caused by the continuous increase of SEI and the destruction of conductive networks.
Disclosure of Invention
One embodiment provides a negative active material for a rechargeable lithium battery that exhibits improved cycle life characteristics and high rate performance.
Another embodiment provides a negative electrode for a rechargeable lithium battery including a negative active material.
Yet another embodiment provides a rechargeable lithium battery including a negative electrode.
One embodiment provides a negative active material for a rechargeable lithium battery, the negative active material including: silicon-carbon composites in which crystalline carbon, silicon particles, and amorphous carbon are agglomerated; and single-walled carbon nanotubes coated on the silicon-carbon composite.
The single-walled carbon nanotubes may be present in an amount of about 0.01wt% to about 0.5wt%, based on 100wt% of the total weight of the negative electrode active material.
The single-walled carbon nanotubes may have an average length of about 0.5 μm to about 10 μm.
The single-walled carbon nanotubes may be coated on the surface of the silicon-carbon composite at a thickness of about 0.2 μm to about 10 μm.
The silicon-carbon composite may include agglomerated products in which crystalline carbon and silicon particles are agglomerated, and amorphous carbon between the agglomerated products and/or covering the surface of the agglomerated products.
Another embodiment provides a negative electrode for a rechargeable lithium battery, the negative electrode comprising: a negative electrode active material layer composed of a negative electrode active material and a binder; and a current collector supporting the anode active material layer.
Yet another embodiment provides a rechargeable lithium battery including: a negative electrode; a positive electrode; and an electrolyte.
The anode active material according to some embodiments may exhibit excellent cycle life characteristics and high rate performance.
Drawings
Fig. 1 is a schematic view illustrating a rechargeable lithium battery according to an embodiment.
Fig. 2 is a graph showing cycle life characteristics of battery cells according to example 1 and comparative examples 1 and 2.
Detailed Description
Hereinafter, embodiments of the present invention are described in detail. However, these embodiments are merely examples, the invention is not limited thereto, and the invention is defined by the scope of the claims.
In the specification, when no definition is provided otherwise, the particle diameter (D50) means an average particle diameter (D50) in which the cumulative volume in the particle distribution is about 50% by volume. The average particle diameter (D50) may be measured by methods known to those skilled in the art, for example, by a particle size analyzer or by transmission electron microscopy images or scanning electron microscopy images. In some embodiments, the measurements are made using a dynamic light scattering measurement device, data analysis is performed, counting the number of particles for each particle size range, whereby the average particle size (D50) value can be readily obtained by calculation.
The negative active material for a rechargeable lithium battery according to an embodiment includes: silicon-carbon composites in which crystalline carbon, silicon particles, and amorphous carbon are agglomerated; and single-walled carbon nanotubes coated with a silicon-carbon composite.
In some embodiments, the coating may have a layer shape, an island shape, or a dot shape. For example, the single-walled carbon nanotube may be of any shape as long as it is positioned on the surface of the silicon-carbon composite. In some embodiments, the single-walled carbon nanotubes may be substantially and continuously coated on the surface of the silicon-carbon composite, for example, to form a layer shape, or the single-walled carbon nanotubes may be discontinuously coated to form an island shape or a dot shape.
The silicon-carbon composite may be an agglomerated product of crystalline carbon, silicon particles, and amorphous carbon, and if described in more detail for it, the silicon-carbon composite may include an agglomerated product in which crystalline carbon and silicon particles are agglomerated, and amorphous carbon between and/or covering the surface of the agglomerated product. In another embodiment, the silicon-carbon composite may include secondary particles in which primary particles of at least one silicon nanoparticle are agglomerated (e.g., an agglomerated product), crystalline carbon coated on the agglomerated product, and amorphous carbon coated on a surface of the agglomerated product.
The amorphous carbon may include soft carbon, hard carbon, mesophase pitch carbide, fired coke, or combinations thereof. The crystalline carbon may comprise natural graphite, artificial graphite, or a combination thereof.
In the silicon-carbon composite, the amount of silicon particles may be about 1wt% to about 60wt% based on the total 100wt% of the silicon-carbon composite, or according to another embodiment, the amount of silicon particles may be about 3wt% to about 60wt% based on the 100wt% of the silicon-carbon composite. In the silicon-carbon composite, the amount of amorphous carbon may be about 20wt% to about 60wt% based on the total 100wt% of the silicon-carbon composite, and the amount of crystalline carbon may be about 20wt% to about 60wt% based on the total 100wt% of the silicon-carbon composite.
The silicon particles may have a particle size of about 10nm to about 30 μm, and according to one embodiment may be about 10nm to about 1000nm, or according to another embodiment may be about 20nm to about 150nm.
The thickness may be appropriately adjusted if the amorphous carbon is positioned to cover the surface of the secondary particles, but may be, for example, about 5nm to about 100nm.
Such a ternary silicon-carbon composite including crystalline carbon, amorphous carbon, and silicon may exhibit improved battery conductivity characteristics due to the inclusion of carbon, and according to an embodiment, pores that may be formed inside the agglomerated product may be filled with carbon, which allows formation of a dense structure, and thus, direct contact of an electrolyte with silicon inside the agglomerated product may be prevented. Collapse of the conductive network caused by volume expansion and contraction during charge and discharge can generally occur. However, the anode active material according to some embodiments may prevent collapse of the conductive network by coating the silicon-carbon composite with single-walled carbon nanotubes, thereby improving cycle life characteristics. This effect of preventing collapse of the conductive network can be achieved only by coating with single-walled carbon nanotubes, and cannot be achieved by coating with multi-walled carbon nanotubes. This is because the lower flexibility of multi-walled carbon nanotubes than single-walled carbon nanotubes does not prevent collapse of the conductive network.
If the silicon-carbon composite is coated with amorphous carbon, the improvement of cycle life characteristics by preventing collapse of the conductive network may be insignificant because the particles may not contact with each other by deterioration due to frequent shrinkage and expansion.
In ternary silicon-carbon composites, single-walled carbon nanotubes may form a continuous conductive network between an inner carbon (e.g., graphite) and an outer carbon (e.g., graphite), and thus, conductivity may be continuously maintained. However, since silicon oxide or single Si does not include internal graphite, coating single-walled nanotubes on silicon oxide (such as SiO x) or single Si cannot prevent collapse of the conductive network (which results in reduction of conductivity due to occurrence of cracks caused by shrinkage and expansion during charge and discharge), and thus, improvement of cycle life characteristics cannot be obtained.
In one embodiment, the amount of single-walled carbon nanotubes may be about 0.01wt% to about 0.5wt%, about 0.02wt% to about 0.5wt%, about 0.05wt% to about 0.5wt%, or about 0.05wt% to about 0.3wt%, based on the total 100wt% of the anode active material. If the amount of the single-walled carbon nanotubes is within this range, segregation (isolation) due to the deterioration of Si can be prevented.
In some embodiments, the single-walled carbon nanotubes act as a conductive material such that, as described above, even if the single-walled nanotubes are included in a much smaller amount than conventional conductive materials, it can impart suitable conductivity to the negative electrode active material.
This is because single-walled carbon nanotubes are used for the negative electrode by coating the silicon-carbon composite, and therefore, carbon nanotubes exist only around the silicon-carbon composite, so that a small amount of carbon nanotubes can impart sufficient conductivity to the negative electrode active material. However, if single-walled carbon nanotubes are simply mixed instead of being coated on the silicon-carbon composite, for example, in the anode active material layer slurry preparation, the single-walled carbon nanotubes are used to mix the silicon-carbon composite, the single-walled carbon nanotubes, and the binder in a solvent, a small amount of single-walled nanotubes having a similar amount to one embodiment may exhibit insufficient conductivity, and thus, high rate performance may be significantly deteriorated.
The single-walled carbon nanotubes may have an average length of about 0.5 μm to about 10 μm, about 0.5 μm to about 5 μm, or about 0.5 μm to about 3 μm. The average length of the single-walled carbon nanotube means not only a complete straight length, but also a length corresponding to the long axis even if the single-walled carbon nanotube existing in the anode active material is bent. If the average length of the single-walled carbon nanotubes is within this range, good contact between particles can be achieved without agglomeration and without segregation in the negative electrode.
In some embodiments, the single-walled carbon nanotubes may be coated on the surface of the silicon-carbon composite at a thickness of about 0.2 μm to about 10 μm, about 0.2 μm to about 8 μm, about 0.2 μm to about 6 μm, or about 0.2 μm to about 4 μm. Coating single-walled carbon nanotubes at this thickness can impart good contact between particles, thereby improving long cycle life characteristics.
Such a negative electrode active material according to the embodiment may be prepared by the following steps.
Silicon particles having a micrometer size are mixed with an organic solvent to prepare a silicon dispersion liquid. The mixing process may be performed by a grinding process to reduce the size of the silicon particles from micrometers to nanometers, thereby obtaining silicon nanoparticles. The milling process may be performed by a sand mill or a ball mill.
The solvent may suitably be a solvent that does not oxidize the silicon particles and that can be easily volatilized, and examples may be isopropanol, ethanol, methanol, butanol, N-methylpyrrolidone, propylene glycol, or a combination thereof.
The mixing ratio of the silicon particles and the organic solvent may be about 70:30 to about 90:10, about 70:30 to about 80:20 by weight. If the mixing ratio of the silicon particles and the organic solvent is satisfied to be within this range, the size of the silicon particles can be rapidly reduced and oxidation can be prevented.
Crystalline carbon is added to the silicon dispersion liquid and mixed. The mixing ratio of silicon and crystalline carbon may be about 90:10 to about 80:20 by weight. If the mixing ratio of silicon and crystalline carbon is within this range, excellent cycle life characteristics can be exhibited.
The crystalline carbon may comprise natural graphite, artificial graphite, or a combination thereof.
The resulting mixture was spray dried to prepare a Si precursor. Spray drying may be performed at about 50 ℃ to about 150 ℃. Spray drying can agglomerate primary particles as silicon nanoparticles to produce secondary particles.
If spray drying is performed in this temperature range, agglomeration of the primary particles may be suitably performed to form the secondary particles.
The Si precursor is mixed with the amorphous carbon precursor.
The mixing ratio of the Si precursor and the amorphous carbon precursor may be about 50:50 to 70:30 by weight. If the mixing ratio of the Si precursor and the amorphous carbon precursor is within this range, amorphous carbon is not included in the final anode active material in an excessive amount, and the amorphous carbon layer is not separately on the surface of the final anode active material, so that a suitable utilization ratio of silicon can be obtained, thereby exhibiting excellent initial efficiency.
The amorphous carbon precursor may include coal pitch, mesophase pitch, petroleum pitch, mesophase pitch, coal base oil, petroleum base heavy oil, or a polymer resin (such as a phenolic resin, furan resin, polyimide resin).
The resulting mixture is heat-treated to produce a heat-treated product.
The heat treatment may be performed at about 800 ℃ to about 950 ℃ for about 1 hour to about 5 hours. The heat treatment positions the amorphous carbon precursor between the primary particles as silicon nanoparticles on the surface portion and surrounds the surface of the secondary particles.
The heat treatment may be performed under an N 2 atmosphere or an argon atmosphere. The heat treatment under the above atmosphere can suppress oxidation of silicon and generation of SiC, and effectively produce amorphous carbon, thereby reducing the resistance of the active material.
The heat treated product, the amorphous carbon precursor, and the single-walled carbon nanotubes may be mixed in a first solvent and a second solvent. The mixing ratio of the heat treated product to amorphous carbon precursor mixture to single-walled carbon nanotubes may be from about 99.99:0.01 to about 99.5:0.5, from about 99.99:0.01 to about 99.7:0.3, from about 99.99:0.01 to about 99.8:0.2, or from about 99.95:0.05 to about 99.8:0.2. The mixing ratio of the heat-treated product and the amorphous carbon precursor may be about 90:10 to 96:4 by weight. The mixing ratio of the heat-treated product and the amorphous carbon precursor in this range allows the inside to be densely filled, and therefore, side reactions with the electrolyte can be reduced, and excellent expansion characteristics can be exhibited.
The first solvent is mixed with the second solvent. The first solvent may include ethanol, methanol, propanol, isopropanol, etc., and the second solvent may include water, ethanol, etc. The mixing ratio of the first solvent and the second solvent may be about 50:50 to about 10:90 by volume. If the mixing ratio of the first solvent and the second solvent is satisfied in this range, the maximum effect for dispersing the powder can be obtained.
Mixing may be carried out for about 1 hour to about 5 hours. If the above mixing is performed for the above time, a coating layer having an appropriate thickness may be formed.
The resulting mixture was dried. Drying may be performed at about 50 ℃ to about 150 ℃. The dried product was heat-treated to prepare a negative electrode active material. According to the heat treatment, an active material in which single-walled carbon nanotubes are coated on the surface of a silicon-carbon composite can be prepared, and an amorphous carbon precursor for coating the single-walled carbon nanotubes is converted into amorphous carbon that may exist on the surface of the silicon-carbon composite.
The heat treatment may be performed at about 800 ℃ to about 950 ℃ for about 1 hour to about 5 hours. The heat treatment may be performed under an N 2 atmosphere or an argon atmosphere. The heat treatment under this condition can suppress oxidation of silicon and generation of SiC, and can firmly adhere the single-walled carbon nanotubes on the surface of the silicon-carbon composite.
The negative electrode according to another embodiment includes a current collector and a negative electrode active material layer on at least one side of the current collector. The anode active material layer may be composed of an anode active material and a binder. For example, the anode active material layer according to one embodiment is composed of an anode active material and a binder, and does not include a conductive material alone. As described above, the single-walled carbon nanotubes included in the anode active material can be used as the conductive material, and thus, additional conductive material is not required in the preparation of the anode active material layer.
Thus, if the amount of single-walled carbon nanotubes based on the total 100wt% of the anode active material layer is calculated and considered as the amount of conductive material, it may be about 0.05wt% to about 0.1wt%, which is a conventional amount of very less than about 1wt% to about 3 wt%.
The anode active material may further include a carbon-based active material together with the active material according to one embodiment. The carbon-based active material may include artificial graphite, natural graphite, or a combination thereof.
If a carbon-based active material is included as the negative electrode active material, the active material and the carbon-based active material according to one embodiment may be included in about 99.9:0.1wt% to about 3:97wt%, about 50:50wt% to about 3:97wt%, or about 40:60wt% to about 4:96 wt%. If the mixing ratio of the active material and the carbon-based active material according to one embodiment is within this range, the volume expansion of the anode active material can be effectively suppressed and the conductivity can be further improved.
In the anode active material layer, the amount of the anode active material may be about 95wt% to about 99wt% based on the total 100wt% of the anode active material layer. The amount of the anode active material refers to the amount of the active material according to one embodiment, and if the anode active material includes the active material according to one embodiment and the carbon-based active material, it refers to the total amount of the mixture of the active material according to one embodiment and the carbon-based active material.
The amount of the binder may be about 1wt% to about 5wt% based on the total 100wt% of the anode active material layer.
The binder improves the binding property of the anode active material particles with each other and the binding property of the anode active material particles with the current collector. The binder may be a non-aqueous binder, an aqueous binder, or a combination thereof.
The non-aqueous binder may be an ethylene propylene copolymer, polyacrylonitrile, polystyrene, polyvinyl chloride, carboxylated polyvinyl chloride, polyvinyl fluoride, polyurethane, polytetrafluoroethylene, polyvinylidene fluoride, polyethylene, polypropylene, polyamideimide, polyimide, or combinations thereof.
The aqueous binder may be styrene-butadiene rubber (SBR), acrylated styrene-butadiene rubber (ABR), acrylonitrile-butadiene rubber, acrylic rubber, butyl rubber, fluoro rubber, ethylene oxide containing polymers, polyvinylpyrrolidone, polypropylene, polyepichlorohydrin, polyphosphazene, ethylene propylene diene copolymers, polyvinylpyridine, chlorosulfonated polyethylene, latex, polyester resin, acrylic resin, phenolic resin, epoxy resin, polyvinyl alcohol, or combinations thereof.
If an aqueous binder is used as the negative electrode binder, the cellulose-based compound may also be used as a tackifier to provide tackiness. The cellulose compounds include one or more of carboxymethyl cellulose, hydroxypropyl methyl cellulose, and alkali metal salts thereof. The alkali metal may be Na, K or Li. The tackifier may be included in an amount of about 0.1 parts by weight to about 3 parts by weight based on 100 parts by weight of the anode active material.
The current collector may include one selected from copper foil, nickel foil, stainless steel foil, titanium foil, nickel foam, copper foam, polymer substrate coated with conductive metal, and combinations thereof, but is not limited thereto.
Another embodiment provides a rechargeable lithium battery including a negative electrode, a positive electrode, and an electrolyte.
The positive electrode includes a current collector and a positive electrode active material layer on the current collector.
The positive electrode active material may include a lithiated intercalation compound that reversibly intercalates and deintercalates lithium ions. In an embodiment, a composite oxide of lithium and one or more metals selected from cobalt, manganese, nickel, and combinations thereof may be used. In some embodiments, a compound represented by one of the following formulas may be used .LiaA1-bXbD1 2(0.90≤a≤1.8,0≤b≤0.5);LiaA1-bXbO2-c1D1 c1(0.90≤a≤1.8,0≤b≤0.5,0≤c1≤0.05);LiaE1-bXbO2- c1D1 c1(0.90≤a≤1.8,0≤b≤0.5,0≤c1≤0.05);LiaE2-bXbO4-c1D1 c1(0.90≤a≤1.8,0≤b≤0.5,0≤c1≤0.05);LiaNi1-b-cCobXcD1 α(0.90≤a≤1.8,0≤b≤0.5,0≤c≤0.5,0<α≤2);LiaNi1-b-cCobXcO2-αTα(0.90≤a≤1.8,0≤b≤0.5,0≤c≤0.5,0<α<2);LiaNi1-b-cCobXcO2-αT2(0.90≤a≤1.8,0≤b≤0.5,0≤c≤0.5,0<α<2);LiaNi1-b-cMnbXcD1 α(0.90≤a≤1.8,0≤b≤0.5,0≤c≤0.5,0<α≤2);LiaNi1-b-cMnbXcO2-αTα(0.90≤a≤1.8,0≤b≤0.5,0≤c≤0.5,0<α<2);LiaNi1-b-cMnbXcO2-αT2(0.90≤a≤1.8,0≤b≤0.5,0≤c≤0.5,0<α<2);LiaNibEcGdO2(0.90≤a≤1.8,0≤b≤0.9,0≤c≤0.5,0.001≤d≤0.1);LiaNibCocL1 dGeO2(0.90≤a≤1.8,0≤b≤0.9,0≤c≤0.5,0≤d≤0.5,0≤e≤0.1);LiaNiGbO2(0.90≤a≤1.8,0.001≤b≤0.1);LiaCoGbO2(0.90≤a≤1.8,0.001≤b≤0.1);LiaMn1-bGbO2(0.90≤a≤1.8,0.001≤b≤0.1);LiaMn2GbO4(0.90≤a≤1.8,0.001≤b≤0.1);LiaMn1-gGgPO4(0.90≤a≤1.8,0≤g≤0.5);QO2;QS2;LiQS2;V2O5;LiV2O5;LiZO2;LiNiVO4;Li(3-f)J2(PO4)3(0≤f≤2);Li(3-f)Fe2(PO4)3(0≤f≤2);LiaFePO4(0.90≤a≤1.8).
In the above chemical formula, a is selected from Ni, co, mn, or a combination thereof; x is selected from Al, ni, co, mn, cr, fe, mg, sr, V, rare earth elements or combinations thereof; d is selected from O, F, S, P or a combination thereof; e is selected from Co, mn or a combination thereof; t is selected from F, S, P or a combination thereof; g is selected from Al, cr, mn, fe, mg, la, ce, sr, V or a combination thereof; q is selected from Ti, mo, mn or a combination thereof; z is selected from Cr, V, fe, sc, Y or a combination thereof; j is selected from V, cr, mn, co, ni, cu or a combination thereof; l 1 is selected from Mn, al or a combination thereof.
In one embodiment, the compound may have a coating layer on the surface, or may be mixed with another compound having a coating layer. The coating layer may include at least one coating element compound selected from the group consisting of an oxide of a coating element, a hydroxide of a coating element, a oxyhydroxide of a coating element, an oxycarbonate of a coating element, and a hydroxycarbonate of a coating element. The compound used for the coating layer may be amorphous or crystalline. The coating elements included in the coating layer may include Mg, al, co, K, na, ca, si, ti, V, sn, ge, ga, B, as, zr or a mixture thereof. The coating layer may be provided by a method using these elements in the compound so as not to adversely affect the properties of the positive electrode active material, for example, the method may include any coating method such as spraying, dipping, or the like, but is not described in more detail since it is well known in the art.
In the positive electrode, the amount of the positive electrode active material may be about 90wt% to about 98wt% based on the total weight of the positive electrode active material layer.
In one embodiment, the positive electrode active material layer may further include a binder and a conductive material. The amounts of the binder and the conductive material may be about 1wt% to about 5wt%, respectively, based on the total amount of the positive electrode active material layer.
The binder improves the binding property of the positive electrode active material particles to each other and the binding property of the positive electrode active material particles to the current collector. Examples of the binder may be polyvinyl alcohol, carboxymethyl cellulose, hydroxypropyl cellulose, diacetyl cellulose, polyvinyl chloride, carboxylated polyvinyl chloride, polyvinyl fluoride, ethylene oxide-containing polymers, polyvinyl pyrrolidone, polyurethane, polytetrafluoroethylene, polyvinylidene fluoride, polyethylene, polypropylene, styrene-butadiene rubber, acrylated styrene-butadiene rubber, epoxy resin, nylon, etc., but are not limited thereto.
Conductive materials are included to provide electrode conductivity, and any electrically conductive material may be used as the conductive material unless it causes a chemical change. Examples of conductive materials may be: carbon-based materials such as natural graphite, artificial graphite, carbon black, acetylene black, ketjen black, carbon fiber, and the like; metal powder or metal fiber metal-based materials including copper, nickel, aluminum, silver, and the like; conductive polymers such as polyphenylene derivatives; or mixtures thereof.
The current collector may be Al, but is not limited thereto.
The electrolyte includes a non-aqueous organic solvent and a lithium salt.
The non-aqueous organic solvent serves as a medium for transporting ions participating in the electrochemical reaction of the battery.
The non-aqueous organic solvent may include carbonate solvents, ester solvents, ether solvents, ketone solvents, alcohol solvents, or aprotic solvents.
The carbonate-based solvent may include dimethyl carbonate (DMC), diethyl carbonate (DEC), dipropyl carbonate (DPC), methylpropyl carbonate (MPC), ethylpropyl carbonate (EPC), methylethyl carbonate (MEC), ethylene Carbonate (EC), propylene Carbonate (PC), butylene Carbonate (BC), and the like. The ester solvents may include methyl acetate, ethyl acetate, n-propyl acetate, dimethyl acetate, methyl propionate, ethyl propionate, propyl propionate, decalactone, mevalonic acid lactone, caprolactone, and the like. The ether solvent may include dibutyl ether, tetraethylene glycol dimethyl ether, diethylene glycol dimethyl ether, dimethoxyethane, 2-methyltetrahydrofuran, tetrahydrofuran, etc. The ketone solvent may include cyclohexanone and the like. The alcohol solvent may include ethanol, isopropanol, etc., and examples of the aprotic solvent may include: nitriles such as r—cn (wherein R is a C2 to C20 linear, branched, or cyclic hydrocarbon, or may include a double bond, an aromatic ring, or an ether linkage); amides such as dimethylformamide; dioxolanes such as 1, 3-dioxolane; sulfolane, and the like.
The nonaqueous organic solvents may be used alone or as a mixture. When the nonaqueous organic solvent is used in a mixture, the mixing ratio can be controlled according to the desired battery performance.
The carbonate-based solvent may desirably comprise a mixture of cyclic carbonates and chain carbonates. The cyclic carbonate and the chain carbonate are mixed together in a volume ratio of about 1:1 to about 1:9. When the mixture is used as an electrolyte, it may have enhanced properties.
The organic solvent may also include aromatic hydrocarbon solvents and carbonate solvents. The carbonate solvent and the aromatic hydrocarbon solvent may be mixed together in a volume ratio of about 1:1 to about 30:1.
The aromatic hydrocarbon organic solvent may be an aromatic hydrocarbon compound represented by chemical formula 1.
[ Chemical formula 1]
In chemical formula 1, R 1 to R 6 are the same or different and are selected from hydrogen, halogen, C1 to C10 alkyl, haloalkyl, and combinations thereof.
Specific examples of the aromatic hydrocarbon-based organic solvent may be selected from benzene, fluorobenzene, 1, 2-difluorobenzene, 1, 3-difluorobenzene, 1, 4-difluorobenzene, 1,2, 3-trifluorobenzene, 1,2, 4-trifluorobenzene, chlorobenzene, 1, 2-dichlorobenzene, 1, 3-dichlorobenzene, 1, 4-dichlorobenzene, 1,2, 3-trichlorobenzene, 1,2, 4-trichlorobenzene, iodobenzene, 1, 2-diiodobenzene, 1, 3-diiodobenzene, 1, 4-diiodobenzene, 1,2, 3-triiodobenzene, 1,2, 4-triiodobenzene, toluene, and the like fluorotoluene, 2, 3-difluorotoluene, 2, 4-difluorotoluene, 2, 5-difluorotoluene, 2,3, 4-trifluorotoluene, 2,3, 5-trifluorotoluene, chlorotoluene, 2, 3-dichlorotoluene, 2, 4-dichlorotoluene, 2, 5-dichlorotoluene, 2,3, 4-trichlorotoluene, 2,3, 5-trichlorotoluene, iodotoluene, 2, 3-diiodotoluene, 2, 4-diiodotoluene, 2, 5-diiodotoluene, 2,3, 4-triiodotoluene, 2,3, 5-triiodotoluene, xylene, or combinations thereof.
The electrolyte may further include ethylene carbonate, vinylene carbonate, or an ethylene carbonate-based compound represented by chemical formula 2 as an additive for improving cycle life.
[ Chemical formula 2]
In chemical formula 2, R 7 and R 8 are the same or different and may each independently be hydrogen, halogen, cyano (CN), nitro (NO 2) or fluoro C1 to C5 alkyl, provided that at least one of R 7 and R 8 is halogen, cyano (CN), nitro (NO 2) or fluoro C1 to C5 alkyl, and R 7 and R 8 are not simultaneously hydrogen.
Examples of the ethylene carbonate-based compound may be difluoroethylene carbonate, chloroethylene carbonate, dichloroethylene carbonate, bromoethylene carbonate, dibromoethylene carbonate, nitroethylene carbonate, cyanoethylene carbonate, fluoroethylene carbonate, and the like. The amount of the additive for improving cycle life characteristics may be used in an appropriate range.
Lithium salts dissolved in organic solvents supply lithium ions to the battery, allowing the rechargeable lithium battery to operate substantially and improving the transport of lithium ions between the positive and negative electrodes. Examples of the lithium salt may include at least one support salt selected from LiPF6、LiBF4、LiSbF6、LiAsF6、LiN(SO2C2F5)2、Li(CF3SO2)2N、LiN(SO3C2F5)2、Li(FSO2)2N( lithium bis (fluorosulfonyl) imide ：LiFSI)、LiC4F9SO3、LiClO4、LiAlO2、LiAlCl4、LiPO2F2、LiN(CxF2x+1SO2)(CyF2y+1SO2)(, where x and y are positive integers, for example, an integer of about 1 to about 20), liCl, liI, liB (C 2O4)2 (lithium bis (oxalato) borate: liBOB), and lithium difluoro (oxalato) borate (lipob). The concentration of the lithium salt may range from about 0.1M to about 2.0M. If the above concentration ranges include lithium salts, the electrolyte may have excellent properties and lithium ion mobility due to optimal electrolyte conductivity and viscosity.
Depending on the type of rechargeable lithium battery, a separator may be disposed between the positive and negative electrodes. The separator may use polyethylene, polypropylene, polyvinylidene fluoride, or a multilayer thereof having two or more layers, and may be a mixed multilayer (such as a polyethylene/polypropylene double-layer separator, a polyethylene/polypropylene/polyethylene triple-layer separator, a polypropylene/polyethylene/polypropylene triple-layer separator, or the like).
Fig. 1 is an exploded perspective view of a rechargeable lithium battery according to an embodiment. The rechargeable lithium battery according to the embodiment is illustrated as a prismatic battery, but is not limited thereto, and may include batteries of various shapes (such as a cylindrical battery, a pouch battery, etc.).
Referring to fig. 1, a rechargeable lithium battery 100 according to one embodiment may include an electrode assembly 40 manufactured by winding a separator 30 disposed between a positive electrode 10 and a negative electrode 20, and a case 50 accommodating the electrode assembly 40. An electrolyte (not shown) may be impregnated in the positive electrode 10, the negative electrode 20, and the separator 30.
Hereinafter, examples of the present invention and comparative examples are described. However, these examples are not to be construed in any way as limiting the scope of the invention.
Example 1
Ethanol solvent and silicon particles having a particle diameter of several micrometers were mixed at a weight ratio of 1:9, and a silicon nanodispersion liquid was prepared by using a sand mill (Netzch, germany).
Artificial graphite was added to the silicon nanodispersion liquid to have a 9:1 weight ratio of silicon to artificial graphite, stirred for the first time and spray dried at 150 ℃ using a spray dryer to prepare Si precursor.
The Si precursor was mixed with the intermediate pitch in a 50:50 weight ratio, and the mixture was heat treated at 900 ℃ under an N 2 atmosphere to prepare a silicon-carbon composite. The silicon-carbon composite includes an agglomerated product as secondary particles in which artificial graphite and silicon nanoparticles are agglomerated, and soft carbon coated on the agglomerated product, the amount of artificial graphite being 40wt% and the amount of amorphous carbon being 20wt% based on the total weight of the silicon-carbon composite.
The prepared silicon-carbon composite, intermediate pitch and single-walled carbon nanotubes (average length: 1 μm to 10 μm) were mixed in a mixed solvent of water and ethanol (3:1 by volume ratio) at a weight ratio of 95:4.95:0.05, stirred for 2 hours, and dried in an oven at 100 ℃ to prepare a dried product.
The resultant dried product was heat-treated at 900 ℃ under an N 2 atmosphere to prepare a negative electrode active material. In the prepared anode active material, the surface of the silicon-carbon composite is coated with single-walled carbon nanotubes at a thickness of 0.2 μm to 0.5 μm.
The negative electrode active material was used as a first negative electrode active material and natural graphite was used as a second negative electrode active material, and the first negative electrode active material, the second negative electrode active material, a styrene butadiene rubber binder, and a carboxymethyl cellulose tackifier were mixed in an aqueous solvent at a weight ratio of 10:87.5:1:1.5 to prepare a negative electrode active material slurry.
The negative electrode active material slurry was coated on a Cu foil current collector, dried, and pressurized under a conventional technique to prepare a negative electrode including the current collector and a negative electrode active material layer on the current collector. The prepared anode active material layer had a load level of 7.0mg/cm 2, and the density of the active material (referred to as anode active material layer) was 1.67g/cm 3.
A rechargeable lithium battery cell (full cell) having a specific capacity of 500mAh/g was fabricated using a negative electrode, a LiCoO 2 positive electrode, and an electrolyte. The electrolyte was used by dissolving 1.5M LiPF 6 in a mixed solvent of ethylene carbonate, ethylmethyl carbonate and dimethyl carbonate (volume ratio of 20:10:70).
Example 2
A negative electrode active material was prepared by the same procedure as in example 1, except that the mixing ratio of the silicon-carbon composite, the intermediate pitch, and the single-walled carbon nanotube was changed to 95:4.9:0.1 by weight. In the prepared anode active material, the surface of the silicon-carbon composite is coated with single-walled carbon nanotubes at a thickness of 0.2 μm to 0.5 μm. As the amount of single-walled carbon nanotubes used increases compared to example 1, the surface area of the silicon-carbon composite coated with the single-walled carbon nanotubes increases.
As the same procedure as in example 1, the negative electrode active material was used as a first negative electrode active material to manufacture a rechargeable lithium battery cell having a specific capacity of 500 mAh/g.
Example 3
A negative electrode active material was prepared by the same procedure as in example 1, except that the mixing ratio of the silicon-carbon composite, the intermediate pitch, and the single-walled carbon nanotube was changed to 95:4.8:0.2 by weight. In the prepared anode active material, the surface of the silicon-carbon composite is coated with single-walled carbon nanotubes at a thickness of 0.2 μm to 0.5 μm. As the amount of single-walled carbon nanotubes used increases compared to example 1, the surface area of the silicon-carbon composite coated with the single-walled carbon nanotubes increases.
By the same procedure as in example 1, the negative electrode active material was used as a first negative electrode active material to manufacture a rechargeable lithium battery cell having a specific capacity of 500 mAh/g.
Comparative example 1
A rechargeable lithium battery cell having a specific capacity of 500mAh/g was manufactured through the same procedure as in example 1, except that the silicon-carbon composite according to example 1 was used as the first negative electrode active material.
Comparative example 2
The prepared silicon-carbon composite, intermediate pitch and acetylene black were mixed in a mixed solvent of water and ethanol (3:1 by volume ratio) at a weight ratio of 95:4.9:0.1, stirred for 2 hours, and dried in an oven at 100 ℃ to prepare a dried product.
The resultant dried product was heat-treated at 900 ℃ under an N 2 atmosphere to prepare a negative electrode active material.
The negative electrode active material was used as a first negative electrode active material and natural graphite was used as a second negative electrode active material, and the first negative electrode active material, the second negative electrode active material, a styrene butadiene rubber binder, and a carboxymethyl cellulose tackifier were mixed in an aqueous solvent at a weight ratio of 10:87.5:1:1.5 to prepare a negative electrode active material slurry. By the same procedure as in example 1, a negative electrode active material slurry was used to manufacture a negative electrode and a rechargeable lithium battery cell having a specific capacity of 500 mAh/g.
Comparative example 3
SiO x (x=1.1), intermediate pitch, single-walled carbon nanotubes (average length: 1 μm to 10 μm) were mixed in a mixed solvent of water and ethanol (3:1 by volume ratio) at a weight ratio of 95:4.5:0.5, stirred for 2 hours, and dried in an oven at 100 ℃ to prepare a dried product.
The resultant dried product was heat-treated at 900 ℃ under an N 2 atmosphere to prepare a negative electrode active material.
As the same procedure as in example 1, the negative electrode active material was used as a first negative electrode active material to manufacture a negative electrode and a rechargeable lithium battery cell having a specific capacity of 500 mAh/g.
Comparative example 4
Using the silicon-carbon composite according to example 1 as a first anode active material and natural graphite as a second anode active material, the first anode active material, the second anode active material, single-walled carbon nanotubes (average length: 1 μm to 10 μm), and a mixture of a styrene butadiene rubber binder and a carboxymethyl cellulose tackifier were mixed in a weight ratio of 9.99:87.5:0.01:2.5 in an aqueous solvent to prepare an anode active material slurry.
By the same procedure as in example 1, a negative electrode active material slurry was used to manufacture a negative electrode and a rechargeable lithium battery cell having a specific capacity of 500 mAh/g.
Comparative example 5
The prepared silicon-carbon composite, petroleum pitch and acetylene black were mixed in a mixed solvent of water and ethanol (3:1 by volume ratio) at a weight ratio of 95:4.9:0.1, stirred for 2 hours, and dried in an oven at 100 ℃ to prepare a dried product.
The resultant dried product was heat-treated at 900 ℃ under an N 2 atmosphere to prepare a negative electrode active material.
The negative electrode active material was used as a first negative electrode active material and natural graphite was used as a second negative electrode active material, and the first negative electrode active material, the second negative electrode active material, a styrene butadiene rubber binder, and a carboxymethyl cellulose tackifier were mixed in an aqueous solvent at a weight ratio of 10:87.5:1:1.5 to prepare a negative electrode active material slurry.
By the same procedure as in example 1, a negative electrode active material slurry was used to manufacture a negative electrode and a rechargeable lithium battery cell having a specific capacity of 500 mAh/g.
Comparative example 6
A negative electrode and a rechargeable lithium battery cell having a specific capacity of 500mAh/g were fabricated by the same procedure as in example 1, except that a multi-walled carbon nanotube (average length: 5 μm to 20 μm) was used instead of using a single-walled carbon nanotube (average length: 1 μm to 10 μm).
Experimental example 1) efficiency characteristics
The rechargeable lithium battery cells according to examples 1to 3 and comparative examples 1to 6 were charged and discharged once at 0.2C, and the ratio of discharge capacity to charge capacity was measured. The results are shown in table 1 as efficiencies.
Experimental example 2) cycle life characteristics
The rechargeable lithium battery cells according to examples 1 to 3 and comparative examples 1 to 6 were charged and discharged 300 cycles at 1C. The ratio of the discharge capacity at each cycle to the discharge capacity at the 1 st cycle was calculated. From the results, the ratio of the discharge capacity at the 200 th cycle to the discharge capacity at the 1 st cycle is shown in table 1 as a capacity retention rate. According to the results, the capacity retention rates when the battery cells according to example 1 and comparative examples 1 and 2 were charged and discharged 300 cycles are shown in fig. 2.
Experimental example 3) high Rate Performance Properties
The rechargeable lithium battery cells according to examples 1 to 3 and comparative examples 1 to 6 were charged and discharged once at 0.2C and charged and discharged once at 2C.
The ratio of the discharge capacity at 2C to the discharge capacity at 0.2C was measured. The results are shown in table 1 as chargeability.
TABLE 1
As shown in table 1 and fig. 2, examples 1 to 3 exhibited excellent efficiency, cycle life characteristics, and charge rate.
However, comparative example 1 using a silicon-carbon composite as the first negative electrode active material exhibited all of low efficiency, cycle life characteristics, and charge rate. Comparative example 2 using the silicon-carbon composite coated with acetylene black as the first negative electrode active material exhibited good efficiency but deteriorated cycle life characteristics and charge rate.
While the present disclosure has been described in connection with what is presently considered to be practical exemplary embodiments, it is to be understood that the invention is not to be limited to the disclosed embodiments, but on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims.
Claims (7)
1. A negative active material for a rechargeable lithium battery, the negative active material for a rechargeable lithium battery comprising:
a silicon-carbon composite in which crystalline carbon, silicon particles, and amorphous carbon are agglomerated; and
Single-walled carbon nanotubes coated on the silicon-carbon composite.
2. The anode active material for a rechargeable lithium battery according to claim 1, wherein the single-walled carbon nanotubes are present in an amount of 0.01wt% to 0.5wt%, based on 100wt% of the total weight of the anode active material.
3. The anode active material for a rechargeable lithium battery according to claim 1, wherein the single-walled carbon nanotube has an average length of 0.5 μm to 10 μm.
4. The negative active material for a rechargeable lithium battery according to claim 1, wherein the single-walled carbon nanotube is coated on the surface of the silicon-carbon composite with a thickness of 0.2 μm to 10 μm.
5. The negative active material for a rechargeable lithium battery according to claim 1, wherein the silicon-carbon composite includes an agglomerated product in which the crystalline carbon and the silicon particles are agglomerated and the amorphous carbon is between the agglomerated products and/or coated on the surface of the agglomerated products.
6. A negative electrode for a rechargeable lithium battery, the negative electrode for a rechargeable lithium battery comprising:
a negative electrode active material layer composed of the negative electrode active material according to any one of claims 1 to 5 and a binder; and
And a current collector supporting the anode active material layer.
7. A rechargeable lithium battery, the rechargeable lithium battery comprising:
the negative electrode of claim 6;
a positive electrode; and
An electrolyte.
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| KR10-2022-0145321 | 2022-11-03 | ||
| KR1020220145321A KR20240063564A (en) | 2022-11-03 | 2022-11-03 | Negative active material for rechargeable lithium battery, negative electrode including same, and rechargeable lithium battery including same |
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| US (1) | US20240170650A1 (en) |
| EP (1) | EP4365987A1 (en) |
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| CN111668472A (en) * | 2020-06-28 | 2020-09-15 | 贝特瑞新材料集团股份有限公司 | Silicon-based composite negative electrode material, preparation method thereof and lithium ion battery |
| KR102271632B1 (en) * | 2021-04-28 | 2021-07-01 | 주식회사 그랩실 | Manufacturing Method of Carbon-Silicon Composite Powder, Carbon-Silicon Composite Powder Manufactured Thereby and Lithium Secondary Battery Comprising the Same |
| CN115132982A (en) * | 2022-06-01 | 2022-09-30 | 万华化学(四川)有限公司 | Preparation method of silicon-based negative electrode material |
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